Preparação de resinas de poliuretana à base de óleo de mamona e dietanolamina

The aim of this work was the preparation of polyols from reactions between castor oil and dietanolamine to increase the hydroxyl content and the network degree in the products to application in electronic devices. The polyols and the mixtures obtained were characterized by nuclear magnetic ressonance. Castor oil (CO) is a natural triglyceride - based polyol possessing hydroxyl groups, which allow several reactions that produce many different products. Among them are the polyurethanes (PU), which have been considered an ideal product for the covering of electricelectronic circuits, due to their excellent electrical, shock-absorbing, solvents resistance and hydrolytic stability properties. About 90% of the fatty acids present in the castor oil are ricinoleic acid (12-hydroxyoleic acid), while the remaining 10% correspond to non-hydroxylated fatty acids, mainly linoleic and oleic acids. The chemical analysis of castor oil indicates a hydroxyl number of 2.7. In this work, a polyol was obtained by the reaction of the CO with diethanolamine (DEA), in order to elevate the hydroxyl value from 160 to 230 or to 280 mgKOH/g, and characterized by nuclear magnetic resonance (NMR) 1H and 13C (Mercury 200). The polyadition of the resulting polyol with isophorone diisocianate (IPDI) was carried out at 60°C, and the reaction kinetics was followed by rheological measurements in a Haake RS150 rheometer. The electrical properties were determined in a HP LCR Meter 4262A, at 1.0 Hz and 10.0 KHz. The chemical analysis showed that the polyols obtained presented hydroxyl number from 230 to 280 mgKOH/g. The polyadition reaction with IPDI produced polyurethane resins with the following properties: hardness in the range from 45 shore A to 65 shore D (ASTM D2240); a dielectric constant of 3.0, at 25°C (ASTM D150). Those results indicate that the obtained resins present compatible properties to the similar products of fossil origin, which are used nowadays for covering electric-electronic circuits. Therefore, the PUs from castor oil can be considered as alternative materials of renewable source, free from the highly harmful petroleum - derived solvents

Temperature dependence and magnetocrystalline anisotropy studies of self-assembled L1(0)-Fe55Pt45 ferromagnetic nanocrystals

Temperature dependence and uniaxial magnetocrystalline anisotropy properties of the chemically synthesized 4 nm L1(0)-Fe55Pt45 nanoparticle assembly by a modified polyol route are reported. As-prepared nanoparticles are superparamagnetic presenting fcc structure, and annealing at 550 degrees C converts the assembly into ferromagnetic nanocrystals with large coercivity (H-C>1 T) in an L1(0) phase. Magnetic measurements showed an increasing in the ferromagnetically ordered fraction of the nanoparticles with the annealing temperature increases, and the remanence ratio, S=M-R/M-S congruent to 0.76, suggests an (111) textured film. A monotonic increase of the blocking temperature T-B, the uniaxial magnetocrystalline anisotropy constant K-U, and the coercivity H-C with increasing annealing temperature was observed. Magnetic parameters indicate an enhancement in the magnetic properties due to the improved Fe55Pt45 phase stabilizing, and the room-temperature stability parameter of 67, which indicates that the magnetization should be stable for more than ten years, makes this material suitable for ultrahigh-density magnetic recording application.(c) 2007 American Institute of Physics.

Iron Oxide Versus Fe55Pt45/Fe3O4: Improved Magnetic Properties of Core/Shell Nanoparticles for Biomedical Applications

In this paper, synthesis of the Fe55Pt45/Fe3O4 core/shell structured nanoparticles using the modified polyol process combined with the seed-mediated growth method is reported. Iron oxide shell thickness was tuned controlling the Fe(acac)(3)/FePt seeds in the reaction medium. Annealing of the core/shell structure leads to iron-rich layer formation around the hard FePt phase in the nanoparticle core. However, the 2 nm Fe3O4 shell thickness seems to be the limit to obtain the enhanced magnetization close to the alpha-Fe and preserving an iron oxide shell after annealing at 500 degrees C for 30 min in a reducing atmosphere. The presence of both the oxide layer on nanoparticle surface and an intermediate iron-rich FePt layer after annealing promote strong decreases in the coercive field of the 2-nm-oxide shell thickness. These annealed nanoparticles were functionalized with dextran, presenting the enhanced characteristics for biomedical applications such as higher magnetization, very low coercivity, and a slightly iron oxide passivated layer, which leads an easy functionalization and decreases the nanoparticle toxicity.

Pd-based catalysts: Influence of the second metal on their stability and oxygen reduction activity

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Surface structure and electronic properties of Pt-Fe/C nanocatalysts and their relation with catalytic activity for oxygen reduction

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Self-assembled FePt nanocrystals with large coercivity: Reduction of the fcc-to-L1(0) ordering temperature

Herein we report the synthesis and properties of Fe55Pt45 nanoparticles, both monodisperse and self-assembled into hexagonal close-packed and cubic arrays of 4.0 +/- 0.2 nm size in an L1(0) structure, obtained by a modified polyol process. The new synthetic route improved the control over the particle composition, thereby reducing the temperature required to convert from face-centered cubic (fcc) to face-centered tetragonal (fct) phase by some 30-50 degrees C without additives. Annealing at 550 degrees C for 30 min converts the self-assembled nanoparticles into ferromagnetic nanocrystals with large coercivity, H-C = 11.1 kOe. Reducing the fcc-to-fct (L1(0)) ordering temperature avoided particle coalescence and decreased the loss in particle positional order without compromising the magnetic properties, as is generally observed when additives are used.

Simultaneous solidification of two catalyst wastes and their effect on the early stages of cement hydration

Two catalyst wastes (RNi and RAI) from polyol production were considered as hazardous, due to their respective high concentration of nickel and aluminum contents. This article presents the study, done to avoid environmental impacts, of the simultaneous solidification/stabilization of both catalyst wastes with type II Portland cement (CP) by non-conventional differential thermal analysis (NCDTA). This technique allows one to monitor the initial stages of cement hydration to evaluate the accelerating and/or retarding effects on the process due to the presence of the wastes and to identify the steps where the changes occur. Pastes with water/cement ratio equal to 0.5 were prepared, into which different amounts of each waste were added. NCDTA has the same basic principle of Differential Thermal Analysis (DTA), but differs in the fact that there is no external heating or cooling system as in the case of DTA. The thermal effects of the cement paste hydration with and without waste presence were evaluated from the energy released during the process in real time by acquiring the temperature data of the sample and reference using thermistors with 0.03 A degrees C resolution, coupled to an analog-digital interface. In the early stages of cement hydration retarding and accelerating effects occur, respectively due to RNi and RAl presence, with significant thermal effects. During the simultaneous use of the two waste catalysts for their stabilization process by solidification in cement, there is a synergic resulting effect, which allows better hydration operating conditions than when each waste is solidified separately. Thermogravimetric (TG) and derivative thermogravimetric analysis (DTG) of 4 and 24 h pastes allow a quantitative information about the main cement hydrated phases and confirm the same accelerating or retarding effects due to the presence of wastes indicated from respective NCDTA curves.

Hexagonal-shaped tin glycolate particles: A preliminary study of their suitability as li-ion insertion electrodes

Tin glycolate particles were prepared by a simple, one-step, polyol-mediated synthesis in air in which tin oxalate precursor was added to ethylene glycol and heated at reflux. Hexagonal-shaped, micron-sized tin glycolate particles were formed when the solution had cooled. A series of tin oxides was produced by calcination of the synthesized tin glycolate at 600-800 degrees C. It was revealed that the micron-sized, hexagonal-shaped tin glycolate now consisted of nanosized tin-based particles (80-120 nm), encapsulated within a tin glycolate shell. XRD, TGA, and FT-IR measurements were conducted to account for the three-dimensional growth of the tin glycolate particles. When applied as an anode material for Li-ion batteries, the synthesized tin glycolate particles showed good electro-chemical reactivity in Li-ion insertion/ deinsertion, retaining a specific capacity of 416mAhg(-1) beyond 50cycles. Ibis performance was significantly better than those of all the other tin oxides nanoparticles (< 160mAhg(-1)) obtained after heat treatment in air. We strongly believe that the buffering of the volume expansion by the glycolate upon Li-Sn alloying is the main factor for the improved cycling of the electrode.

Mechanical properties of vulcanized natural rubber nanocomposites containing functional ceramic nanoparticles

Rubber nanocomposites containing different concentrations of ferroelectric and paramagnetic nanoparticles were fabricated. Nanostructures of ferroelectric potassium strontium niobate and paramagnetic nickel-zinc ferrite were synthesized using a modified polyol method. The nanoparticle characterization was carried out by transmission electron microscopy and X-ray diffraction, showing that the materials were produced with nanometer dimensions, specific crystallinity and microstrain. Mechanical tests such as hardness type Shore A, stress-strain and compression resistance were performed. They showed that increasing the concentration of nanoparticles enhance the rigidity of vulcanized films of natural rubber and this change is more pronounce for the nanocomposites formed with ferrite nanoparticles, likely due to the effect of its morphological and surface properties. © 2013 by American Scientific Publishers.

Influence of the concentration of polyols on the rheological and spectral characteristics of guar gum

Polyols are widely used as sugar substitutes and provide texture to foods. Guar gum has many applications in food industry such as increasing product viscosity and improving texture. Knowledge of rheological properties of gum/polyol systems is important to permit replacing sugar while maintaining product texture. In this work, rheological properties of 0.1, 0.5 and 1 g/100 g guar solutions containing 10 and 40 g/100 g of maltitol, sorbitol, or xylitol were studied. The behavior of these mixtures was evaluated by steady and oscillatory shear measurements, and after a freezing/thawing cycle. Apparent viscosity of guar solutions increased with addition of polyols and with the increase in their concentrations, except for 40 g/100 g sorbitol addition to 1 g/100 g guar gum, in which the apparent viscosity decreased. Addition of polyols also increased the dynamic moduli of the systems. In mixtures of guar with 40 g/100 g polyol, the phase angle (δ) was below unity, but was dependent on frequency, which is characteristic of concentrated solutions with a certain degree of structuring. FTIR spectroscopy was studied to provide information on possible interactions between guar gum and polyols. Analyses carried out after freezing/thawing showed no changes in the viscoelastic behavior of the solutions. © 2013 Elsevier Ltd.

Influence of potassium and sodium nutrition on leaf area components in Eucalyptus grandis trees

Background and Aims: Recent studies showed a positive tree response to Na addition in K-depleted tropical soils. Our study aimed to gain insight into the effects of K and Na fertilizations on leaf area components for a widely planted tree species. Methods: Leaf expansion rates, as well as nutrient, polyol and soluble sugar concentrations, were measured from emergence to abscission of tagged leaves in 1-year-old Eucalyptus grandis plantations. Leaf cell size and water status parameters were compared 1 and 2 months after leaf emergence in plots with KCl application (+K), NaCl application (+Na) and control plots (C). Results: K and Na applications enhanced tree leaf area by increasing both leaf longevity and the mean area of individual leaves. Higher cell turgor in treatments +K and +Na than in the C treatment resulting from higher concentrations of osmotica contributed to increasing both palisade cell diameters and the size of fully expanded leaves. Conclusions: Intermediate total tree leaf area in treatment +Na compared to treatments C and +K might result from the capacity of Na to substitute K in osmoregulatory functions, whereas it seemed unable to accomplish other important K functions that contribute to delaying leaf senescence. © 2013 Springer Science+Business Media Dordrecht.

Preparação e caracterização de óxido de zinco nanoestruturado

Pós-graduação em Ciência e Tecnologia de Materiais - FC

Caracterização dielétrica de partículas nanométricas e nanoestruturadas de óxido de niobato da família tetragonal tungstênio bronze com estequiometria K'Sr IND. 2' N'b IND. 5' 'O IND. 15'

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Comportamento reológico de gomas guar e xantana na presença de polióis

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Síntese e caracterização elétrica de compósitos poliméricos condutores com o poliuretano derivado de óleo de mamona como matriz

Pós-graduação em Ciência dos Materiais - FEIS